Cyclohexyl isocyanate → HCID 178418526、化合物

HRID 3796

反応式

HRID 3796 の反応式
[CH:1]1([N:7]=[C:8]=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:10][C:11]1[CH:27]=[CH:26][C:14]([CH2:15][N:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][SH:25])[CH2:18][CH2:17]2)=[CH:13][CH:12]=1>C(Cl)Cl>[ClH:10].[ClH:10].[CH:1]1([NH:7][C:8](=[SH:25][CH2:24][CH2:23][CH2:22][N:19]2[CH2:20][CH2:21][N:16]([CH2:15][C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:27][CH:26]=3)[CH2:17][CH2:18]2)[OH:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 18502Cyclohexyl isocyanateHCID 137311173-[4-(4-Chlorobenzyl)piperazin-1-yl]propanethiol

生成物 1

HCID 178418526HCID 178418526、化合物収率 100.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1.0 g of cyclohexyl isocyanate, 2.1 g of 3-[4-(4-chlorobenzyl)piperazin-1-yl]propanethiol and 10 ml of methylene chloride was stirred at room temperature overnight and then concentrated in vacuo. The residue crystallized upon standing. The product was recrystallized from aqueous ethanol, dissolved in ether, and the ethanol solution was dried (magnesium sulfate). The salt was then precipitated with ethereal hydrochloric acid and recrystallized twice from aqueous ethanol to give 1.2 g (30% of theory) of N-cyclohexyl-S-{3-[4-(4-chlorobenzyl)piperazin-1-yl]propyl}thiocarbamate dihydrochloride as a white crystalline solid, M.p. >165° C. (dec.).

後処理

  1. concentrationconcentrated in vacuo
  2. customThe residue crystallized
  3. customThe product was recrystallized from aqueous ethanol
  4. dissolutiondissolved in ether
  5. dry with materialthe ethanol solution was dried (magnesium sulfate)
  6. customThe salt was then precipitated with ethereal hydrochloric acid
  7. customrecrystallized twice from aqueous ethanol

出典と根拠

ORDレコード
ord-9d1937c896e54cb4b8977e4368ead391
出典データセット
uspto-grants-1988_02
特許番号
US04722926

関連ノート

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